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' bilityao UNITED snares PATENT onnrou re all 'tv hob m may concern:

- Be'it known that LEMIL- OOLLETT," a subjeot of' the *King of Norway, of- Christian-ia, Norway; ha e invented-certain new and use =ful Improvements in- Processes for the Mans u facture ot Ammonium Perchlorate; and I do hereby declare the-following to beafull, clear, and-exact "description of the invention; s chas will enable-others skilled in the art to which itf'appertains to'make and use the; same; 1

Perchlorate of ammonium is usually inanutactured' lathe. inannerthat perchlorate of s'od-iumasreacted upon with an ammonium ammoniunn In all these known reactions thenature of' the salts contained in the solu- I tion wil-l be such-that the diflerence in soluconnected with the separation of th S lt from each other and with the production of a' pure ammonium perchlorate." 'As' a matter'oi coursethfe-sai'd difiieultiesalsoinvolve bonate of;sodium aftreatnient with a'ni- 4011s-rnon1um -bicarbonateor ammonia and cars.

bonic': acldg this latter process being} applied to the sodium nitratebearing-solution remaining after the precipitation "of the am lnonium perchlorate;so. that a precipitation 4550f bicarbonate ofjsodium and forniati'onyof nitrate 'ot ammonium takeiplacein the soluti'ong; which then: could be reactedupon; with furthervquantities of sodiumiperchlorate. The process may be carried out in the fol- 5"0- lowing' mann'er ii Solutions containing suitable percentages V 'ofiso'diumi perchlorate and ammonium 'ni-' trla-tegr es ectively'are brought togetherg with theefe's'itt that ar perchlorate-pf ammoniumgis' thezyarious salts is comparatively 20--*sma1 1; great difiiculties beingconsequently- Emmottm, or onnizsrrnmn; NORWAY.

' PROCESS FOR THEMANUFAC RE or AMMonIUMrERcriLonATE;

formed whichis precipitated in ample quantities,' the said'salt being-of a'comparatively low solubility, while the other-*salt's contained in thesolution in question are easily soluble- This reaction between nitrate of 'annnoniun and perchlorate of sodium as such is already known; According 'toa known process asat present practised "the Specification ofLetters Patent; =7 P tg t 19 7 A uc'ationmea-november144918: s riai-nofaeasaa" mother liquor containing-nitrates ofi an nionium and o f sodiuni' as well as the perchlorate of sodium and ain'inonium is evaporated and the substances contained therein "separated from each other b fractional crys-v talliza'tion. This evaporation and crystalli za-tion is very troublesome and involves high costs. On the one hand the plant: necessary for carrying the operation into effect is ex pen'slve for the reason that large quantities.

of water must be eliminated, which'requires a voluminous apparatus and on the other hand" special expensive materials for the evaporation apparatus structure must" be usedbecauseordinary ironis attacked b the liouids in ouestioir being therefore not a--pplicable.-- The apparatuses accordingly wil1 become very expensive as regards their construction as well as in operation, and the necessary expenses incident to amortization and repair. 1 The other OPGI-atIOI1S---COIHP11S ing the separation of the substances by crystallization are alsovery laborious andthe costs of the crystallization, filtration" 1 washing, conveyanceand other manipulations consequently :bec'ome very high as regards the plant aswellyas the expenses: for-wages, interest, repair :andamortization.

All these difiicu'lties and" complications which attach a to the hitherto employed methods for themanufacture of ammonium perchlorate and which are ftjh'e source of such high expenses havebroughtit about p'ortance to the modern industry "of explosive s, has not attained tlie significance which 7 it would possess if the:manufacturingjcosts were lower. All the idi'fii'culties-and'jcost referred to abovecan be avoided however when thedescribed reaction between NaClO; and NI-LNO in accordance-*witkthe pres- "ent invention is combined with another known process, the I mother liquor obtained by the reaction being treated. in suchfainiam an that the evaporatican is avoided; It -is known (cfr. Lunge: Avmnomlak 4th Ed.

1900, pages 257 and 258) to produce ammonium nitrate from sodium nitrate in solution by the addition of NH and CO Hereby NaHCO is precipitated and NILNO is-retained in the solution.

.NH NO it would be expectedthat an addi- The mother liquor from the reaction between NaClO, and NH NO substantially contains NaNO By the addition ofainmonium carbonate or carbonic acid to this mother liquor NaHCO will be precipitated,

the content o-fNaNO in the solution being converted into NH NO The mother liquor containing besides NaNO also considerable quantities of ammonium salts '(NH,ClO

tion of NH and CO would result in the vprecipitation of ammonium salts together with NaHCO The surprising observation has been made however that this does not take .place. The explanation of this fact may be found in the formation of certain insoluble double compounds of the salts contained in the solution. However that may be, the fact is that a considerableproportion of the sodium content ofthe mother liquor" is precipitated as NaHCO so that the N0 of the mother liquor is again combined with the NH as NH NO It is thus possible in a very simple manner and without any evaporation to produce a solution of nitrate of V ammonium, which may again be reacted upon with further quantities, of NaClO Of coursethis solution of NILNQ, contains 7 some other salts of Na and NH, combined with C10 NO and CO but this fact is withoutimportance to the use of the liquid as an NH NO solution for the reaction with NaClO The fact is that when this latter substance is added in a suitable manner eitherin adissolved state or as a solid to the regenerated NI-L NO solution, NI-LCIO, is

. precipitated as fine pure crystals, which are tial constituent is heated NaClO,

easily filtered and washed.

An embodiment of the invention is described in the following by way of example: 1 A liquid containing NHQNO as a substanand supplied with in a solid condition (or in the form of a more or less concentrated solution if this is desirable) whereupon the solution is V cooled. NILCIO is precipitated and is then 7 separated from the liquid- (no evaporation being required). The liquid is thensu plied with NH and 00,, whereby NaHCS precipitates (still no evaporation necessary). The slgierposed liquid which now. contains NH N 3 isagaln supplied with NaClO as above described whereby NI-LCIO precipitates. This treatment is continued with alternative precipitation of NI LCIO and N aHCO respectlvely the same water being repeatedly used for the solution so that all evaporation (except of the water necessary for the washing operation); and. all costs and difliculties connected with such evaporation i are avoided.

Besides the advantages mentioned above, the present process also involves the advantage over theusual methodsiin that either a pure sodium bicarbonate .or soda 'is obtained as a by-productin a simple and efficient way,

the said product being as is known, an article in demand and for which there is a ready market. 'By the usual method of manufacturing'NH C1O that is from NaClO and NI-LCI sodium chlorid is obtained as a .by- -product.- ,As is known, however, this'substance is of .a low commercial value, this being particularly. so in the present instance I because it is difficult to obtain a product free from NHfilC) and other ammonium salts. Acontent of these latter salts renders the product unsuitable for use in foods and as a material for electrolytical conversion into NaClO, because the ammonium salts present.

are by electrolysis converted into NCl which is a highly explosive substance and its manipulation consequently connected with danger. The electrolysis of such sodium .chlorid is for these-reasonsnot practicable.v

It is obvious therefore that the above derscribed combination of operationinvolves a great technical and economical improvement with regard to thetechnical execution of the process as well as regarding theeflicient'utilization of the employed products.

I claim: v r

1. Process for the, manufacture of ammonium perchlorate comprising the step of reacting upon sodium perchlorate with ammonium nitrate in combination with the step of reacting upon the resulting sodium nitrate in the presence of ammonium bicarbonate.

2. Process for the manufacture of ammonium perchlorate comprising thestep of" reacting upon-sodium'perchlorate with ammonium nitrate in combination with thestep of reacting upon the resultin sodium nitrate in the presence of carbonmonia. I v

3. Processfor the. manufacture'of ammonium perchlorate comprising the step of 5. Process for the manufacture :of am-s monium perchlorate consisting .in' reacting upon ammonium nitrate with'sodium perchlorate 1n thepresence of water, separating the precipitated ammonium perchlorate ioxid and am- I nitrate contained in the saidsolution with fromthe solution, reacting upon thesodium In testimony that I claim the foregoing as my invention, I have signed my name in presence of two subscribing Witnesses.

EMIL COLLETT.

ammonia and carbonic acid, separating the precipitated sodium bicarbonate and adding a further quantity of sodium perchlorate to the solution to precipitate ammonium per chlorate.

Witnesses MAGENS BUGGE, MATHILDE ENGEHEKEN.

Copies of this patent may he obtained forfive cents each, by addressing the commissioner ot Patents,

I Washington, DJO. 

